The effect of zirconium dioxide addition on crystal structure of sol-gel TiO2 mesoporous films and powders has been investigated by means of Raman spectroscopy, X-Ray diffraction, and Atomic force microscopy. Zirconium incorporation (up to 30 mol%) into TiO2 lattice resulted in the formation of Ti1-xZrxO2 solid solution with anatase structure for the binary powders has been proved. Appearance of tetragonal ZrO2 phase was observed for the samples with high zirconium content. (C) 2011 Elsevier By. All rights reserved.